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A. FRANK 8v N. CARO.

' PROCESS 0F MAKING CYANIDS.

' No. 590,217. Patented sept. 21,1897.

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PROCESS 0F MAKING CYANIDS.

No. 590,217. I Patented Sept. 21,1897.

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i Wwdd/ v .7W/jeden@ 6207?/ v NTTED Y STATES PATENT rrrcn,

ADOLPH FRANK, OF CHARLOTTENBURG, AND -NIKODEM CARO, OF BERLIN,

' GERMANY.

'PROCESS oF MAKING CYANIDS.

SPECIFICATION forming part of Letters Patent No. 590,217, dated September 21, 1897.

Application iiled November 5, 1895. Serial No. 568,023.. (No specimens.) Patented in Belgium August l0, 1895, No. 116,953, and in Luxembqurg August 11, 1895,1To. 2,346.

To @ZZ whom it may concern:

Beit known that we,ADoLPH FRANK,resid ing at Charlottenburg, and NIKODEM CARO, residing at Berlin, Germany, have invented certain new and useful Improvements in and Relating to the Production of Cyanogen Combinations, (for which Letters Patent have been obtained in Belgium, No. 116,953, bearing date August 10, 1895, and in Luxemburg,

' Io No. 2,346, bearing date August 11, 1895;) and we do hereby declare the following to be a full, clear, and exact description of the invention, such as will enable others skilled in the art to which it appertains to make and use the same, reference being had to the accompanying drawings, and to letters of reference marked thereon, which form a part of this specification.

Our invention has relation to the produczo tion of cyanogen combinations; and it has for its obj cota novel process of producing the same.

According to the statement ofMoissan, (Comptes Rendus, 1894, p. 503,) the passing 2 5 of nitrogen over the heated carbids of calcium, barium, and strontium does not result in a reaction or combination. We have discernl ered, however, that nitrogen is taken up by carbids in presence of steam in a closed ves- 3o sel, as in a tubular or other retort or the like, the carbids having previously been heated to a temperature approximating that of red heat. Theformation of the cyanids takes place in the manner described, whether the carbids 3 5 of the metals of the alkaline earths-such as calciun1,barum, strontiu in, and magnesiumor the metals of the alkalies-such as potassium, sodium, or lithium-are employed, this being likewise the case when mixtures of 4o these carbids are used or when the carbids contain any other substance, as an alkali (soda or potash) or an alkaline earth (lime, baryta, strontia, or magnesia) or the salts of the alkalies or alkaline earths. The mixture of carbids maybe effected by means of the dierent carbids themselves, or by forming the carbids from raw materials, as the oxids and of tubular form.

or carbonates of the alkalies and alkaline earths, or the free metals by admixture Wit-h carbon in any well-known or desired manner, or by mixing the respective carbidsV of the metals of the alkaline earths or a mixture thereof with an alkali or alkalies or a salt or salts thereof.

In the production of carbids from the free metals and carbon practical experiments have shown it to be advisable to subject the same to the required high temperature in a closed retort or vessel, especially when metals are used that volatilize at the said temperatureas potassium, sodium,and magnesium, as well as the zinc chemically allied or similar to the latter-in order to produce the carbids by the action of the vapors of the metals upon the carbon, the reaction in the production of sovdium carbid, for instance, taking place according to the following equation:

Cx-I-Nay I CxNay.

We have further` discovered that when iron or iron combinations are mixed with the substances from which the carbids are produced and the mixture is treated as described the corresponding cyanogen combinations can be Obtained. Y

We will now describe the mode of carrying out our invention by the following examples: First. Comminuted barium carbid is lplaced in a refractory vessel, preferably of flrefclay The retort'is provided with a suitable inlet and an outlet for the induction and eduction of the nitrogen or gaseous matter. The nitrogen (which may be air freed from its oxygen) is saturated with steam, and this may be convenientlyeffected by simply passing the nitrogen through water, which latter is converted into steam within the heated retort. After the retort and itscontents have been heated to aboutared heat the moisture-laden nitrogen is' caused to flow or is forced into the same. For a charge of from fifteen to seventeen kilos barium carbid from two to two and one-half cubic meters of nitrogen will be required, which is preferably forced into the retort at a moderate pressure l cyanid, for instance, takes place according to and at such a rate of speed that the operation will be concluded in about two hours. The material in the retort is then allowed to cool and treated with water. From the unconverted carbid acetylene is evolved,which may be collected separately, while barium cyanid goes over into solution and is recovered from the liquid in a well-known manner.

In the production of barium cyanid, as described, the reaction takes place in accordance with the following equation:

Second. Calcium carbid when treated as just described does not give very favorable results, while excellent results are obtained with a mixture of this carbid and barium carbid, also with a mixture of calcium and sodium carbid, the latter being obtained in the usual manner from soda-lime and carbon. The reaction product obtained by the action of nitrogen and steam upon the described mixtures can likewise be washed out with water, as described in the first example, the acetylene evolved being collected and the cyanogen combination separated from the solution. The latter can be readily effected by adding to the solution an acid, preferably carbonio acid, whereby cyanid of hydrogen is driven out, the latter gas being then brought into contact with the oxid of the metal the cyanogen salt of which it is desired to obtain. The desired cyanid may also be obtained from its solution by double decomposition for instance, by addition of an alkali carbonate-- whereby the cyanid of a metal of the alkaline earths is converted into the cyanid of the corresponding metal of the alkalies which remains in solution and into an alkaline-earth carbonate.

Third. The result obtained by the treatment described in the iirst example of barium as well as calcium carbid may be greatly improved by mixing the carbids or a mixture thereof with a caustic alkali or an alkali carbonate and then subjecting the same to the action of heat, nitrogen, and steam, as described in said first example, the product of the reaction being then treated as described in example 2.

Fourth. Carbids of the metals of the alkalies, as those of potassium, sodium, and lithium, yield per se, or when mixed, even in presence of an alkaline earth, as lime, baryta, strontia, magnesia, or their salts, the corresponding cyanids when treated as described in the iirst example, the cyanids being obtained from the reaction products by washing out with water and then separating the same from their solution in a well-known manner.

The reaction in the production of potassium the following equation:

K,c,+N,:2KcN.

The temperature most favorable to the production of the described cyanogen combinations is a dark-red heat, the action of the nitrogen being very sluggish or slow at lower temperatures,while at materially-higher temperatures the yield is reduced by reason of a partial decomposition taking place.

For the best utilization of the nitrogen a number of retorts can be arranged in battery through which the gas is successively forced, and mcans provided whereby any one or more of such retorts may be cut out without interrupting the operation of the remaining retorts, thereby making the operation a continuous one.

Any suitable apparatus may be employed in carrying out my invention, and in the accompanying drawings I have shown an apparatus of simple construction for the purpose.

Figure l is ahorizontal section on line c w of Fig. 2, and Fic'. 2 a vertical section on line fr y of Fig. l.

In the iigurcs of drawings, B indicates the fuel-grate; O, a flue leading from said grate to the heating-chamber E, said iiue formed by extending the fire-bridge D nearly to the upper wall of the apparatus, openings d being formed in said nre-bridge controlled by suitable dampers s, whereby the heat and products of combustion can be led into the heating-chamber at different levels, as may be required in heating the retortsA A, which latter, as shown, are arranged vertically in said heating-chamber. The retorts are provided with charging and discharging covers or caps L L' at their upper and lower ends, which ends project, respectively, above and below the top and y bottom of the heatingchamber E, and are connected at those points with gas-supply and exhaust-pipes K and Kl, respectively, the products of combustion escaping from chamber E to a stack H through a suitable flue F. Any desired number of retorts A may be arranged within the heating-chamber. I have shown four such retorts as an example.

It will be observed that the described process is of the simplest nature, capable of being carried out at a low temperature (dark-red heat) as compared with the temperatures required in the known processes, while the yield of cyanogen combinations greatly exceeds that ot any other process known to us.

Having thus described our invention, what we claim as new, and desire to secure by Letters Patent, is-

l. In a process for producing cyanogen combinations, subjecting a described carbid IOO IIO

combinations7 subjecting a described carbid of a suitable inet-al, as a metal of the alkalies, to the action of heat and nitrogen in the prese-nce of steam and of a feriferous substance, substantially as described.

In testimony that We claim the foregoing as our invention We have signed our naines in presence of two subscribing Witnesses.

ADOLPH FRANK. NIKODEM CARO.

Vitnesses:

RICHARD SCHMIDT, v W. HAUPT. 

